Abstract:The electrochemical copolymerization of aminoterephthalic acid (ATA) and o-aminophenol (OAP) was carried out on platinum electrodes in acidic medium. The obtained material, poly(ATA-co-OAP), can be deposited by cyclic scanning of the potential in a wide potential range and shows significant electroactivity. However, it was observed that a copolymer with less overoxidation defects is obtained at inversion potentials where only OAP monomer (and not ATA monomer) is oxidized. The successful incorporation of unoxid… Show more
“…A third peak at around 402 eV is also observed in all the potentials. This peak can be associated with more oxidized nitrogen species [47,48]. These oxidized nitrogen species increase significantly in the SWCNT modified at 1.8 V, in agreement with what has been observed in other amine-containing molecules, electrochemically attached on different materials surfaces [49,50].…”
Section: 3xps Analysis Of P and N Species On Electrochemically Modsupporting
confidence: 87%
“…7 presents the XPS N1s spectra for the SWCNT modified at different upper potential limits, showing different species depending on the applied potential. The region between 398.5 and 400.1 eV can be assigned to neutral amines and imines species, respectively, generated during the oxidation of 4-APPA which are also observed in PANI, and are in agreement with the formation of oligomer/polymeric chains [40,46,47]. A third peak at around 402 eV is also observed in all the potentials.…”
Section: 3xps Analysis Of P and N Species On Electrochemically Modsupporting
Single Wall Carbon Nanotubes (SWCNTs) have been successfully functionalized by electrochemical oxidation in presence of 4-aminophenyl phosphonic acid (4-APPA).Electrochemical modification has been performed by cyclic voltammetry using different upper potential limits, producing the incorporation of N and P functionalities on SWCNT through polymerization reactions, although some covalent attachment cannot be discarded. Electrochemical oxidation in presence of CNT produces polymerization of 4-APPA, what has been related to the interaction between monomer and the CNT surface.The voltammograms of the functionalized SWCNT show different well-defined redox processes that are maintained at high pH. Raman spectroscopy shows that the structure of the SWCNT is maintained even at high potentials suggesting that oxidation selectively occurs in the 4-APPA monomer favoring polymer chain growth. The degree of modification of SWCNT can be easily controlled by selecting the electrochemical conditions.
“…A third peak at around 402 eV is also observed in all the potentials. This peak can be associated with more oxidized nitrogen species [47,48]. These oxidized nitrogen species increase significantly in the SWCNT modified at 1.8 V, in agreement with what has been observed in other amine-containing molecules, electrochemically attached on different materials surfaces [49,50].…”
Section: 3xps Analysis Of P and N Species On Electrochemically Modsupporting
confidence: 87%
“…7 presents the XPS N1s spectra for the SWCNT modified at different upper potential limits, showing different species depending on the applied potential. The region between 398.5 and 400.1 eV can be assigned to neutral amines and imines species, respectively, generated during the oxidation of 4-APPA which are also observed in PANI, and are in agreement with the formation of oligomer/polymeric chains [40,46,47]. A third peak at around 402 eV is also observed in all the potentials.…”
Section: 3xps Analysis Of P and N Species On Electrochemically Modsupporting
Single Wall Carbon Nanotubes (SWCNTs) have been successfully functionalized by electrochemical oxidation in presence of 4-aminophenyl phosphonic acid (4-APPA).Electrochemical modification has been performed by cyclic voltammetry using different upper potential limits, producing the incorporation of N and P functionalities on SWCNT through polymerization reactions, although some covalent attachment cannot be discarded. Electrochemical oxidation in presence of CNT produces polymerization of 4-APPA, what has been related to the interaction between monomer and the CNT surface.The voltammograms of the functionalized SWCNT show different well-defined redox processes that are maintained at high pH. Raman spectroscopy shows that the structure of the SWCNT is maintained even at high potentials suggesting that oxidation selectively occurs in the 4-APPA monomer favoring polymer chain growth. The degree of modification of SWCNT can be easily controlled by selecting the electrochemical conditions.
“…These species are usually present in PANI chains (see Figure S9) [18]. The third component (N 3 ) appearing at a binding energy close to 401.6 eV could be related to the presence of nitrogen at a higher oxidation state, specifically to positively charged nitrogen in polymeric films generated during electrooxidation [42,45]. On the other hand, N1s spectra in Figure 8 for PANI-2APPA and PANI-4APPA copolymers could be deconvoluted into three main contributions in all cases, which could be assigned to different nitrogen species.…”
In this study, the phosphonation of a polyaniline (PANI) backbone was achieved in an acid medium by electrochemical methods using aminophenylphosphonic (APPA) monomers. This was done through the electrochemical copolymerization of aniline with either 2- or 4-aminophenylphosphonic acid. Stable, electroactive polymers were obtained after the oxidation of the monomers up to 1.35 V (reversible hydrogen electrode, RHE). X-ray photoelectron spectroscopy (XPS) results revealed that the position of the phosphonic group in the aromatic ring of the monomer affected the amount of phosphorus incorporated into the copolymer. In addition, the redox transitions of the copolymers were examined by in situ Fourier-transform infrared (FTIR) spectroscopy, and it was concluded that their electroactive structures were analogous to those of PANI. From the APPA monomers it was possible to synthesize, in a controlled manner, polymeric materials with significant amounts of phosphorus in their structure through copolymerization with PANI.
“…In poly-PD and poly(ANI-co-PD) those contributions are more important as consequence of the over oxidation in the polymer chains during the synthesis, in comparison with PANI/ V 2 O 5 composites (see Figure S1). [27,28] However, when vanadium is incorporated (see Figure 1B,D) contributions at lower binding energies at around 516.4 and 517.1 eV are observed, related with the vanadium species with oxidation states of V +4 and V +5 , respectively. [29,30] Eventually, the pristine nanoparticles of vanadium employed show a ratio O/V = 2.5, in agreement with the ratio found in the V 2 O 5 , thus only V +5 is present in the sample (see Figure S3).…”
Hybrid materials consisting of aniline (ANI) and/or 2-aminodiphenylamine (PD) in the presence of V 2 O 5 nanoparticles were synthesized by in-situ chemical oxidative polymerization in one-step. Physicochemical and electrochemical characterization confirmed that in the structure of the composites, intercalation between the polymer chains and the V 2 O 5 slabs occurs. Optical properties study shows that the optical band gap of poly(ANI-co-PD)/V 2 O 5 is lower than poly-PD/ V 2 O 5. Thermal stability of the composites by thermogravimetric analysis was evaluated. Composites showed electrochemical activity with improved electrontransfer of the redox species in the polymer observed by cyclic voltammetry. These results highlight the great influence of the V 2 O 5 sheets and the polymer composition on the hybrid materials formation and properties.
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